US9175041B2ActiveUtilityA1

Crystal structures of dolastatin 16, dolamethylleuine and dolaphenvaline, and methods for preparing dolamethylleuine and dolaphenvaline

Assignee: PETTIT GEORGE RPriority: Apr 25, 2011Filed: Apr 25, 2012Granted: Nov 3, 2015

Est. expiryApr 25, 2031(~4.8 yrs left)· nominal 20-yr term from priority

Inventors:George R. Pettit Thomas Smith Jun Xu Delbert Herald

C07C 227/18A61K 38/00G16C 10/00C07K 7/54C07K 5/0205G06F 19/701

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Abstract

The present invention relates to the crystal structures of dolastatin 16, dolamethylleuine and dolaphenvaline. The present invention also relates to processes for preparing dolamethylleuine and dolaphenvaline. The present invention further relates to computer readable medium with crystal structural data and/or information stored thereon.

Claims

exact text as granted — not AI-modified

What is claimed is: 
     
       1. A crystal comprising dolastatin 16: 
       
         
           
           
               
               
           
         
         wherein said crystal is in space group P2(1); and said crystal has unit cell dimensions of a=10.844 (5) Å, b=16.133 (5) Å, c=16.050 (5) Å, α=90.000 (5°), β=104.062 (5°), γ=90.000 (5°), V=2720.4 (17) Å 3 . 
       
     
     
       2. A crystallizable composition comprising dolastatin 16, wherein the crystallizable composition forms a crystal of dolastatin 16 that is of X-ray diffraction quality and wherein said crystal is in space group P2(1); and said crystal has unit cell dimensions of a=10.844 (5) Å, b=16.133 (5) Å, c=16.050 (5) Å, α=90.000 (5°), β=104.062 (5°), γ=90.000 (5°), V=2720.4 (17) Å 3 . 
     
     
       3. A crystal of dolastatin 16 having the X-ray crystal structure of  FIG. 1  and wherein said crystal is in space group P2(1); and said crystal has unit cell dimensions of a=10.844 (5) Å, b=16.133 (5) Å, c=16.050 (5) Å, α=90.000 (5°), β=104.062 (5°), γ=90.000 (5°), V=2720.4 (17) Å 3 . 
     
     
       4. A method of obtaining a crystal of dolastatin 16, wherein said crystal is in space group P2(1); and said crystal has unit cell dimensions of a=10.844 (5) Å, b=16.133 (5) Å, c=16.050 (5) Å, α=90.000 (5°), β=104.062 (5°), γ=90.000 (5°), V=2720.4 (17) Å 3 , the method comprising the steps of:
 (a) combining dolastatin 16 with a crystallization solution to produce a crystallizable composition; and 
 (b) subjecting the crystallizable composition to conditions that promote crystallization, thereby obtaining said crystal.

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